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Preparation method of ultra-high metal loading hydrogenation catalyst

A technology of hydrogenation catalyst and loading capacity, which is applied in the field of preparation of ultra-high metal loading hydrogenation catalyst, and can solve problems such as clogging, decrease in catalyst specific surface area, and decrease in catalyst activity

Active Publication Date: 2019-02-12
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But limited by the carrier γ-Al 2 o 3 Due to the limitation of pore volume and particle packing density, the hydrogenation catalyst prepared by metal solution impregnation method has better pore structure and larger specific surface area, but the loading of active metal is about 25-35wt%; When the load is increased, the active metal will block the pores of the catalyst, thereby reducing the specific surface area of ​​the catalyst and reducing the activity of the catalyst.

Method used

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  • Preparation method of ultra-high metal loading hydrogenation catalyst
  • Preparation method of ultra-high metal loading hydrogenation catalyst
  • Preparation method of ultra-high metal loading hydrogenation catalyst

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preparation example Construction

[0019] figure 1 It is a flow chart of the preparation method of the metal loading hydrogenation catalyst in the embodiment of the present invention, such as figure 1 Shown, the preparation method of the metal-loaded hydrogenation catalyst provided by the invention comprises the following steps:

[0020] S101: Depositing an aluminum source modifier on a carrier. Wherein, the aluminum source modifier is a composition of one or more of aluminum isopropoxide, aluminum chloride and aluminum nitrate; the carrier is a silica carrier, and the Si / Al atomic ratio is 5-25.

[0021] S102: Mixing the metal, the organic complexing agent and deionized water. Among them, the metal includes the main component and the auxiliary component; the main component is Mo and W of the VIB group, and the auxiliary component is Co and / or Ni of the VIII group; the aluminum source modifier is aluminum isopropoxide, chlorine Composition of one or more of aluminum chloride and aluminum nitrate; Ni(Co) / (M...

Embodiment 1

[0029] Weigh 50g of large pore volume SiO 2 Put it in a beaker, add 500ml of n-hexane, then weigh 11.3g of aluminum isopropoxide, Si / Al=15, dissolve it with a small amount of n-hexane under stirring and add it to the beaker; then add 1500ml of n-hexane, and continue stirring at room temperature 24 hours. Filter, wash with a large amount of n-hexane, dry at 127°C for 8 hours, and then heat up to 580°C at a rate of 2°C / min and calcinate for 6 hours to obtain an aluminum source-modified silica carrier, which is designated as S-1.

[0030] Weigh 50g of large pore volume SiO 2 Put it in a beaker, add 500ml of absolute ethanol, then weigh 7.4g of anhydrous aluminum chloride, Si / Al=5, dissolve it with a small amount of absolute ethanol under stirring and add it to the beaker; then add 1500ml of absolute ethanol, Stirring was continued at room temperature for 24 hours. Filter, wash with a large amount of absolute ethanol, dry at 127°C for 8 hours, and then heat up to 580°C at a rat...

Embodiment 2

[0034] The water absorption rate of measuring carrier S-1 is 1.8ml / g, takes by weighing the silicon dioxide carrier S-1 of 100g aluminum source modification, 110.7g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O), 33.6g ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O), 46.9g ammonium metatungstate ((NH 4 ) 6 h 2 W 12 o 40 ·XH 2 O) and 53.4g citric acid (C 6 h 8 o 7 ·H 2 O). Dissolve nickel nitrate with an appropriate amount of water first, add citric acid until completely dissolved, then add ammonium molybdate and ammonium metatungstate, continue stirring at 60°C until completely dissolved to form a NiMoW co-impregnation solution, and finally make the solution volume up to 200ml. The catalyst was prepared by an equal-volume impregnation method. After the impregnation, it was dried at 100°C for 6 hours, calcined at 450°C for 4 hours, and the heating rate was 2°C / min to obtain catalyst A1. The constant volume V satisfies V=θm; where, θ is the water absorption rate of the ca...

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Abstract

The invention relates to a method for preparing an ultra-high metal loading hydrogenation catalyst, which includes the following steps: depositing an aluminum source modifier on a carrier; mixing metal, organic complexing agent and deionized water; and impregnating the mixed product. onto a carrier deposited with an aluminum source modifier; the carrier impregnated with the mixed product is dried and then roasted; where the main metal components are Mo and W from group VIB, and the auxiliary components are Co and / or from group VIII. or Ni; the aluminum source modifier is one or more combinations of aluminum isopropoxide, aluminum chloride and aluminum nitrate; the pore volume of the carrier on which the aluminum source modifier is deposited is 1.5 to 3.0ml / g , the specific surface area is 400~800m2 / g, and the proportion of 15~20nm pore diameter is greater than 50%. The preparation method of an ultra-high metal loading hydrogenation catalyst provided by the present invention not only significantly improves the catalyst activity by increasing the metal loading, but also makes the catalyst have a better pore structure and a larger specific surface area; and simplifies the preparation process of the catalyst. , reducing the preparation cost of hydrogenation catalysts with high metal content.

Description

technical field [0001] The invention relates to the technical field of petrochemical industry, in particular to a method for preparing a hydrogenation catalyst with an ultra-high metal loading capacity. Background technique [0002] In recent years, with people's increasing attention to environmental quality and the improvement of environmental protection awareness, higher requirements have been put forward for the production of vehicle fuels, especially vehicle diesel sulfur content and cetane number. National V and National The quality index of VI diesel oil requires ultra-low sulfur content (<10μg / g) in vehicle diesel. The cetane number of national V and national VI standard vehicle diesel should be greater than 51 and 53 respectively. To increase the cetane value of diesel Values ​​require deep hydrodearomatics. Currently, the hydrogenation process is the most effective way to achieve this goal, and high-performance hydrogenation catalysts are the key. [0003] The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/888B01J21/12B01J32/00B01J35/10C10G45/50C10G45/08
CPCC10G45/08C10G45/50B01J23/002B01J23/8885B01J2523/00C10G2300/308C10G2300/307C10G2300/202C10G2300/1059C10G2300/1055B01J35/615B01J35/617B01J35/638B01J2523/31B01J2523/41B01J2523/68B01J2523/69B01J2523/845B01J2523/847
Inventor 柴永明郭阳刘宾董斌刘晨光殷长龙张孔远李奕川谢坤左萌赵晋翀
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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